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Abstract:

A heteromorphic granule comprising lysine free base and a lysine salt is
disclosed. A fertilizer composition is set forth having cores containing
an acid salt of a basic amino acid and effective amounts of first and
second layer coatings coated sequentially to the surface of each core. A
method for using the heteromorphic granule as a fertilizer and/or an
animal feed is provided.

Claims:

2. The heteromorphic granule of claim 1 wherein the lysine salt is
selected from the group consisting of lysine hydrochloride and lysine
sulfate.

3. The heteromorphic granule of claim 1 wherein the granule has a core of
the dried lysine freebase surrounded by a coating of a dried lysine salt.

4. The heteromorphic granule of claim 1 wherein the granule is comprised
of a dried lysine salt admixed with dried free lysine base wherein the
lysine salt comprises between 10 percent and 80 percent of the granule.

5. The heteromorphic granule of claim 1 wherein the granule has an inner
core containing a first fraction of a dried lysine salt, a medial layer
coating the core comprised of a dried lysine freebase, and an outer layer
coating the medial layer comprised of a second fraction of dried lysine
salt.

6. The heteromorphic granule of claim 1 wherein the granule has a core of
a dried lysine salt surrounded by a coating of a dried lysine freebase.

11. The heteromorphic granule of claim 7 wherein the granule has a core of
a dried lysine freebase surrounded by a coating of the dried threonine.

12. The heteromorphic granule of claim 7 wherein the granule has a core of
the dried threonine surrounded by a coating of a dried lysine salt
admixed with dried lysine freebase.

13. A heteromorphic granule comprising at least two components, at least
one of which is dried lysine freebase at 10-80% the weight of the
granule, and wherein the granule absorbs less than 10% water when exposed
to a temperature of 10 degrees Celsius to 50 degrees Celsius and a
humidity of between 30% and 91% relative humidity for a period of 24 to
168 hours.

14. The composition of any one of claims 1-13 wherein the granule further
includes at least one inorganic compound comprising at least one element
selected from the group consisting of nitrogen, phosphorous, potassium,
magnesium, manganese, iron and zinc.

15. A method comprising:fermenting a microorganism to produce a
fermentation broth containing a cell mass and a soluble lysine
fraction;separating the cell mass from the solubilized lysine freebase
fraction;purifying the solubilized lysine fraction to obtain a lysine
enriched fraction;neutralizing a portion of the lysine enriched fraction
with a mineral acid to produce a lysine salt;spray agglomerating at least
one of the solubilized lysine freebase fraction and the lysine enriched
fraction with the lysine salt to produce heteromorphic lysine granules.

16. The method of claim 15 wherein the lysine salt is dried before being
spray agglomerated with at least one of the solubilized lysine freebase
fraction and the lysine enriched fraction.

17. The method of claim 15 wherein the lysine salt is a solubilized lysine
salt fraction which is spray agglomerated with at least one of the
solubilized lysine freebase fraction and the lysine enriched fraction.

18. The method of claim 15 wherein the lysine salt is selected from the
group consisting of lysine hydrochloride and lysine sulfate.

19. The method of claim 15 further including adding a nutritive mineral or
mineral salt to the spray agglomeration.

20. A method of use of a composition comprising the heteromorphic granules
according to any one of claims 1-14 for at least one application selected
from the group consisting of a fertilizer and an animal feed.

21. A feed additive for ruminants, which consists essentially of cores
containing an acid salt of a basic amino acid, and a first coating layer
and a second coating layer coated sequentially on the surface of each
core, wherein said first coating layer contains at least one first
coating agent selected from the group comprising salts of a basic amino
acid, freebase of an amino acid, alkali metal salt, nitrogen source,
phosphate source, potassium source, and the second coating layer contains
as a second coating agent selected from the group comprising salts of a
basic amino acid, freebase of an amino acid, alkali metal salt, nitrogen
source, phosphate source, potassium source.

22. The feed additive according to claim 21, wherein the first coating
agent is at least one amino acid selected from the group comprising
methionine, leucine, isoleucine and tryptophan.

23. The feed additive according to claim 21, wherein the second coating
agent is at least one amino acid selected from the group comprising
methionine, leucine, isoleucine, valine, cysteine, tryptophan, threonine
and phenylalanine.

24. The heteromorphic granule of any one of claims 1-14 wherein the
granule has an irregular non-spherical morphology and a particle size
distribution ranging from 10 μm to 800 μm and wherein a powder
consisting of the heteromorphic granules is characterized as free flowing
when exposed to a temperature of 10 degrees Celsius to 50 degrees Celsius
and a humidity of between 30% and 91% relative humidity for a period of
24 to 168 hours.

25. The heteromorphic granule of any one of claims 1-14 having multiphase
morphology of roughly spherical shape that comprises alternating layers
of lysine freebase and at least one of lysine hydrochloride and threonine
arranged concentrically.

26. A powder comprising the heteromorphic granule of any one of claims
1-14 wherein the granules in the powder have a morphology selected from
the group consisting of: a core-shell morphology, a gradient morphology,
an "ice-cream cone" morphology, a "raspberry" morphology and a
"salt-and-pepper" morphology.

27. A fertilizer composition, which consists essentially of cores
containing an acid salt of a basic amino acid, and effective amounts of a
first coating layer and a second coating layer coated sequentially on the
surface of each core, wherein said first coating layer contains at least
one first coating agent selected from the group comprising salts of a
basic amino acid, freebase of an amino acid, alkali metal salt, nitrogen
source, phosphate source, potassium source, and the second coating layer
contains as a second coating agent selected from the group comprising
salts of a basic amino acid, freebase of an amino acid, alkali metal
salt, nitrogen source, phosphate source, potassium source.

28. The fertilizer composition according to claim 27, wherein the first
coating agent is at least one amino acid selected from the group
comprising methionine, leucine, isoleucine and tryptophan.

29. The fertilizer composition according to 27, wherein the second coating
agent is at least one amino acid selected from the group comprising
methionine, leucine, isoleucine, valine, cysteine, tryptophan, threonine
and phenylalanine.

31. The fertilizer composition according claim 27 wherein the N--P--K
ratio is selected from the group comprising 1-1-1, 2-1-1, 3-1-1, 3-2-1 or
2-3-1.

Description:

CROSS-REFERENCE TO RELATED APPLICATION

[0001]This application claims the benefit of U.S. Patent Application Ser.
No 60/995,561 filed Sep. 27, 2007. The entire contents of U.S. Patent
Application Ser. No. 60/995,561 is incorporated by reference into this
application

[0003]The following background material includes information that may be
useful in understanding the present teaching. It is not an admission that
any of the information provided herein is prior art, or material, to the
presently described or claimed disclosures, or that any publication or
document that is specifically or implicitly referenced is prior art.

[0004]L-lysine is an essential amino acid that is supplied as a feed
supplement for both monogastric and ruminant animals lysine feed
supplements are commercially supplied in essentially three forms--as
dried granules of lysine-HCl salt (often called merely lysine HCL), as a
dried broth from a fermenter from which the lysine was made by bacterial
fermentation (often referred to as lysine sulfate because the predominant
form of the lysine from a dried broth is as a sulfate salt) and finally
as free lysine that is supplied as liquid solution to be sprayed onto
animal feed as a supplement (often called lysine freebase). There are
minor variations in some compositions of these three forms of lysine
feed. For example, lysine HCl granules may include minor amounts of
anti-caking agents to improve flow properties, dried lysine sulfate may
or may not include the bacterial cell mass from the fermentation broth,
and lysine freebase may be supplied in different liquid concentrations.

[0005]Each of the three forms of commercially available lysine feed
supplements have advantages and disadvantages. Some advantages of lysine
HCl are that the dried granules are relatively speaking, pure,
inexpensive to ship, easy to control in terms of production
specifications, and have low hygroscopic character. The major
disadvantages are that it is costly to make because it requires
purification and crystallization of lysine from a fermentation broth, and
only 80% of the weight of the product is lysine--the remainder being the
HCl. The major advantage of lysine sulfate is that it is simplest to
make, however, its disadvantages are that the product has variable
composition because it is simply a dried fermentation broth, and for the
same reason is relatively impure, with typically no more than 50% of the
dry weight of the product being lysine. The major advantages of lysine
freebase are that the lysine product in solution high purity, and the
ease of shipping and handling a liquid. The major disadvantages of lysine
freebase is that because it is provided as a solution, shipping costs on
a lysine content basis are higher than for the other dry products, and
that dedicated mixing equipment is needed to dispense the product onto
animal feed.

[0006]lysine may also be used in the agricultural industry as a
fertilizer. The nitrogen content of lysine is sufficient for practical
use as fertilizer, which has the advantages of being organic,
biodegradable and a source of nutrition for soil microbes. lysine alone,
however, lacks other mineral ingredients such as potassium and phosphate
that are often added to a fertilizer. The same advantages and
disadvantages of the three forms of lysine mentioned above apply equally
when the product is used as a fertilizer.

[0007]Although it would seem desirable to sell lysine freebase as a dried
product to lower shipping and production costs, from a commercial
standpoint such a product is not desirable because lysine freebase is
much more hygroscopic than lysine HCl or lysine sulfate, causing the
product to cake, swell and loose the free flowing properties that make a
dried product easy to manage and dispense. There is therefore, a need in
the art to provide a dried lysine feed product that has at least some of
the advantages of lysine freebase but without the disadvantages that make
such a product undesirable.

[0008]The present disclosure addresses this need and others that will be
apparent from the disclosure that follows.

SUMMARY

[0009]Described herein are various embodiments of heteromorphic lysine
granules and mixtures. These embodiments are a combination of dried
lysine freebase blended with--or agglomerated into a layered structure
with--various amounts of lysine HCl, salt particles, other amino acids or
other crude sources of lysine. These heteromorphic granules and mixtures
offer many of the advantages of lysine HCl in terms of ease of use and
low hygroscopic character, while providing at least a portion of the
advantages of lysine freebase in terms of purity and ease of production.
The teachings of this disclosure are concerned with new lysine products
that incorporate dried lysine freebase. Currently there are two forms of
soft lysine widely accepted in the marketplace: (1) lysine HCl, which is
a crystalline and dried salt of lysine, and (2) liquid lysine, which is a
concentrated solution of substantially pure lysine freebase in water. It
is a generally accepted fact that lysine freebase is simpler to
manufacture (on a pure lysine basis) because the manufacture of salts of
lysine such as lysine HCl requires several additional processing steps.
However, these advantages are somewhat offset by additional
transportation costs incurred in delivering liquid lysine. Additionally
the handing of lysine freebase requires an investment in additional
infrastructure for the customer. Hence, in general lysine freebase is
viable for only large volume customers.

[0010]The ability of a dried form of lysine freebase that is free flowing
and does not exhibit significant caking properties is important aspect of
the process for increasing the application of lysine freebase for small
volume customers.

[0011]In one aspect a composition comprising a granule of a dried lysine
salt admixed with dried free lysine freebase wherein the lysine salt
comprises between 10 percent and 80 percent of the granule is described.
In certain embodiments the composition may comprise a granule that has a
core of a dried lysine freebase surrounded by a coating of a dried lysine
salt.

[0012]In another aspect a composition comprising a granule having an inner
core containing a first fraction of a dried lysine salt, a medial layer
coating the core comprised of a dried lysine freebase, and an outer layer
coating the medial layer comprised of a second fraction of dried lysine
salt is described. In certain embodiments, the composition may comprise a
granule of a dried threonine admixed with dried free lysine freebase
wherein the lysine freebase comprises between 10 percent and 80 percent
of the granule. In certain other embodiments the composition may comprise
a granule of a dried threonine admixed with dried lysine salt wherein the
lysine salt comprises between 10 percent and 80 percent of the granule.
In certain other embodiments a composition comprising a granule of a
dried threonine admixed with dried lysine salt and dried free lysine
freebase wherein the lysine components, comprise between 10 percent and
80 percent of the granule is described.

[0013]In another aspect a method is described where a fermentation is done
with a microorganism to produce a fermentation broth containing a cell
mass and a soluble lysine fraction, followed by a method to separate the
cell mass from the solubilized lysine fraction; followed by purifying the
solubilized lysine fraction and neutralizing a portion of the solubilized
lysine fraction with a mineral acid to produce a lysine salt. Certain
embodiments may additionally include a method for spray agglomerating the
solubilized lysine fraction and lysine salt to produce heteromorphic
lysine granules.

[0014]In another aspect a composition is described which comprises a
granule that has a core of a dried lysine salt surrounded by a coating of
a dried lysine freebase. In certain embodiments the composition may also
comprise a granule that has a core of a dried lysine freebase surrounded
by a coating of a dried threonine freebase. In certain other embodiments
the composition may comprise a granule that has a core of a dried
threonine freebase surrounded by a coating of a dried lysine salt.

[0015]In other aspects are described compositions comprising dried lysine
freebase that absorbs less than 10% water when exposed to a temperature
of 10 degrees Celsius to 50 degrees Celsius and a humidity of between 30%
and 91% relative humidity for a period of 24 to 168 hours.

[0016]In certain embodiments lysine and salts of lysine may be produced by
a fermentation of Corynebacterium glutamicum. In certain other
embodiments the threonine may be produced by Escherichia Coli
fermentation.

[0017]In certain yet other aspects a method is described for the use of a
composition comprising granules of dried lysine freebase coated with a
lysine salt for at least one application selected from the group
consisting of a fertilizer and an animal feed. Certain embodiments may
include a feed additive for ruminants, that consists essentially of cores
containing an acid salt of a basic amino acid, and effective amounts of a
first coating layer and a second coating layer coated sequentially on the
surface of each core, wherein said first coating layer contains at least
one first coating agent selected from the group comprising salts of a
basic amino acid, freebase of an amino acid, alkali metal salt, nitrogen
source, phosphate source, potassium source, and the second coating layer
contains as a second coating agent selected from the group comprising
salts of a basic amino acid, freebase of an amino acid, alkali metal
salt, nitrogen source, phosphate source, potassium source.

[0018]In certain embodiments the first coating agent may be at least one
amino acid selected from the group comprising methionine, leucine,
isoleucine and tryptophan. In certain embodiments the second coating
agent is at least one amino acid selected from the group comprising
methionine, leucine, isoleucine, valine, cysteine, tryptophan, threonine
and phenylalanine. Other embodiments include a free-flowing powder of a
lysine freebase, having irregular nonspherical morphology coated with a
layer of salt of lysine and a particle size distribution ranging from 10
μm to 800 μm. Certain other embodiments include a free-flowing
powder of a salt of lysine, having irregular nonspherical morphology
coated with a layer of lysine freebase and a particle size distribution
ranging from 10 μm to 800 μm. Certain yet other embodiments include
a free-flowing power of a lysine freebase, having multiphase morphology
of roughly spherical shape that comprises alternating layers of lysine
freebase and lysine hydrochloride or threonine arranged concentrically,
In certain embodiments a free-flowing power of a salt of lysine, having
multiphase morphology of roughly spherical shape that comprises
alternating layers of lysine freebase and a salt of lysine or threonine
arranged concentrically are described. Certain embodiments may include
heteromorphic granules of lysine or threonine that have a morphology
selected from core-shell, gradient, ice-cream cone, raspberry, salt and
pepper or onion. In certain embodiments the granules may have more than
one type of morphologies. Certain yet other embodiments may include
heteromorphic granules of lysine or threonine that are additionally
co-coated with mineral salts. In certain embodiments, the salts may
provide nitrogen, phosphorous and potassium nutrients to the granules.
Additional embodiments describe heteromorphic granules that have an
N--P--K ratio of 1:1:1. In some embodiments the N--P--K ratio may be
2-1-1, 3-1-1, 3-2-1 or 2-3-1. Also described herein are processes for
producing the heteromorphic granules described herein.

[0019]Additional embodiments include producing the heteromorphic granules
at a first location, and transporting the composition to a second
location. In certain other embodiments the first location and the second
location may be countries.

[0020]Additional embodiments describe lysine granules that are produced by
a micro-organism that is not genetically modified. Yet additional
embodiments include a facility operatively configured to perform the
process or make the compositions described herein.

DETAILED DESCRIPTION

[0021]Definitions

[0022]Prior to describing the present invention in detail, certain terms
that have plain meanings generally understood by those of ordinary skill
in the art are nevertheless defined herein to better distinguish nuances
in meaning intended by the inventors. It is understood that the
definitions provided herein are intended to encompass the ordinary
meaning understood in the art without limitation, unless such a meaning
would be incompatible with the definitions provided herein, in which case
the provided definitions control.

[0023]"About" when used with reference to a numerical expression, means
the greater of: (1) the degree of error of a typical instrument or
process used to measure the items referenced by the expression, (2) plus
or minus 10% of the stated value; or (3) with respect to a range, near
enough to the minima or maxima of the range so as not to have any
noticeable difference in form or function in comparison to an element
exactly at the stated minima or maxima.

[0024]"Dry" or "Dried" means a material has a moisture content of less
than 15% wt/wt, or has been treated to reduce the moisture content of the
material to less than 50% the moisture content of the same material not
so treated.

[0025]The term "lysine" means the amino acid lysine
(C6H14N2O2) and salts or derivatives thereof, and
includes all isomers of lysine (i.e., L-lysine, D-lysine, and any mixture
of L- and D-lysine).

[0026]For convenience of expression, the term "dryer" will hereafter be
used to describe any suitable drying means such as a spray dryer, drum
dryer, tunnel dryer, rotary dryer, tray dryer, and spray granulator.

[0028]The term "separation" when applied to a fermentation broth will
hereafter be used to describe the separating of a lysine fermentation
broth into two fractions: a cell rich lysine broth and a substantially
cell free lysine broth. Any suitable separating means or combination of
separating means may be used. Separation may be achieved by means of
filtration (e.g. ultra- and microfiltration), and mechanical methods such
as centrifugation, hydroclones, rotary vacuum filters, settling tanks,
depth filters and decanting.

[0029]The terms "evaporation" and "evaporated" will hereafter be used to
describe the removal of water by evaporation, which is carried out in the
approximate temperature range of between 140 degree F. and 214 degree F.,
with a pressure between 2.9 psia and 11 psia (vacuum).

[0032]The term "lysine freebase" means the amino acid lysine in the
absence of a neutralizing salt.

[0033]The term "material containing lysine" will hereafter be used to
describe any material of manufacture that contains any form of lysine
alone or in combination with other materials and is commercially used at
least in part for delivery of lysine. Suitable forms of lysine in a
material containing lysine include, but are not limited to, a lysine
fermentation broth with or without cell mass, a dried lysine fermentation
broth, lysine hydrochloride, lysine sulfate, and/or lysine freebase.

[0034]The term "final lysine feed supplement" will hereafter be used to
describe a commercially available material containing lysine f having a
lysine of a purity within a range between about 15% and 80% lysine,
measured as a percent of lysine by weight of material, and which is used
to supplement feed for a non-human animal.

[0044]FIG. 10 is a schematic is of granulated lysine feed product
comprising threonine 40 core surrounded by a lysine hydrochloride 20
shell which in turn is also surrounded by another shell of lysine
freebase 10.

[0045]FIG. 11 is a schematic is of granulated lysine feed product
comprising lysine hydrochloride 20 core surrounded by a threonine 40
shell which in turn is also surrounded by another shell of lysine 10
freebase.

[0046]FIG. 12 is a schematic is of granulated lysine feed product
comprising lysine freebase 10 core surrounded by a lysine hydrochloride
20 shell which in turn is also surrounded by another shell of threonine
40.

[0047]FIG. 13 is a schematic of granulated lysine feed products with
different pluralities of cores of lysine freebase 101 lysine
hydrochloride 20 or threonine 40 shells on cores of lysine freebase 10,
lysine hydrochloride 20 or threonine 40 or a plurality thereof.

[0048]FIG. 14 is a schematic of representative particle morphologies.

[0049]FIG. 15 is a flow chart, showing the principal steps in a process
for making an amino acid feed supplement in which a salt of an amino acid
is mixed with a freebase amino acid to produce a substantially dust free,
free flowing granular amino acid product.

[0050]FIG. 16 is a flow chart, showing the principal steps in a process
for making an amino acid feed supplement in which a salt of an amino acid
is mixed with a freebase amino acid to produce a substantially dust free,
free flowing granular amino acid product.

DESCRIPTION OF EXEMPLARY EMBODIMENTS

[0051]One aspect of this teaching provides a free flowing dried amino acid
product containing lysine that exhibits reduced caking properties in
comparison to dried lysine freebase alone. Various embodiments focus on a
heteromorphic lysine granule product with greater pourability over lysine
freebase alone and higher lysine content than lysine salt products alone.
In certain embodiments the granules are a combination of lysine freebase,
and a salt of lysine, and/or with threonine or a salt of threonine. Other
embodiments may include pure free dry freebase lysine or blends of lysine
freebase and a salt of lysine such as lysine hydrochloride with a
concentration of lysine freebase ranging from 10 percent by weight to 100
percent by weight.

[0052]Pure dry lysine freebase may be used to make the granules. "Pure" in
this context means at least 90% of the dry weight of the material is
lysine freebase. As the proportion of lysine freebase is increased the
cost savings associated with manufacturing the product are expected to be
higher. Blending of a salt of lysine is usually required to modify the
handling characteristics of the blend so that the final product is easy
to handle and package. One especially desired aspect is improvement in
the flowability, pourability and anticaking properties of the blends
during packaging, storing and handling.

[0053]In one aspect lysine granules of "onion morphology" or core-shell
morphology may be produced. Onion morphology may be a multiphase
morphology of roughly spherical shape that comprises alternating layers
of different forms of lysine or threonine arranged concentrically,
typically with all layers being of similar thickness. In an embodiment
the different forms of lysine may comprise lysine freebase, lysine
hydrochloride, lysine sulfate or lysine cell broth. In another embodiment
threonine or different forms of threonine may be used. In yet another
embodiment, various mineral salts that provide a nutritive value in
animal feed may also be used. Such salts may include a solid potassium
salt, such as potassium chloride, mixed with an ammonium
nitrate-containing liquid or solid salt phase that also contains ammonium
phosphate, or to which ammonium phosphate may also be added.

[0054]Various morphologies of lysine granules may be of the type shown in
non-limiting embodiments depicted in FIGS. 1-12. For instance, as
depicted in FIG. 1, a roughly spherical shape morphology may comprise a
core of lysine hydrochloride 20 surrounded by a shell of lysine freebase
10 and a second shell of lysine hydrochloride 20. An alternative
embodiment, as depicted in FIG. 2, may be a roughly spherical shape
comprising a core of lysine freebase 10 surrounded by a shell of lysine
hydrochloride 20 and a second shell of lysine freebase 10. The inner
cores may in certain embodiments, be about 400 microns in diameter. In
certain other embodiments the granules may be between 10 microns to 800
microns. In another non-limiting embodiment, a core of lysine freebase 10
may be surrounded by a shell of lysine hydrochloride 20 as depicted in
FIG. 3, or a core of lysine hydrochloride 20 may be surrounded by a shell
of lysine freebase 10 as depicted in FIG. 4.

[0055]One embodiment of the onion morphology may comprise a core of lysine
freebase 10 coated with a single outer layer (shell) of lysine
hydrochloride 20 as depicted in FIG. 5, resulting in improved flow
properties.

[0056]Another aspect may comprise an heteromorphic lysine containing
granule that includes threonine. In one embodiment of this aspect, a core
of threonine 40 is surrounded by a shell of lysine freebase 10 as
depicted in FIG. 6. In another embodiment of this aspect, a core of
lysine freebase 10 may be surrounded by a shell of threonine 40 as
depicted in FIG. 7. Another non-limiting embodiment may comprise a core
of threonine 40 surrounded by a shell of lysine hydrochloride 20 as
depicted in FIG. 8. Yet another non-limiting embodiment may comprise a
core of lysine hydrochloride 20 surrounded by a shell of threonine 40 as
depicted in FIG. 9.

[0057]Yet another aspect may comprise a core of threonine 40 surrounded by
a layer of lysine hydrochloride 20 surrounded by a shell of lysine
freebase 10 as depicted in FIG. 10. In one particular embodiment, as
depicted in FIG. 11, the core may be lysine hydrochloride 20 surrounded
by a layer of threonine 40 surrounded by shell of lysine freebase 10. In
another embodiment, as depicted in FIG. 12, the core may be lysine
freebase 10, surrounded by a layer of lysine hydrochloride 20 surrounded
by a shell of threonine 40.

[0058]In another aspect, lysine granules of a "raspberry morphology" or
"cauliflower morphology" may be produced. In such case the granules thus
obtained have a distorted or irregular morphology, which resembles that
of "raspberries" or of "Cauliflowers", rather than spherical beads. Such
morphologies of the final product may also in another embodiment, have an
irregular nonspherical morphology and a particle size distribution
ranging from 10 μm to 800 μm.

[0059]In one embodiment, the raspberry morphology as depicted in FIG. 13A
includes several cores of irregular granules of lysine hydrochloride 20
surrounded by a shell of lysine freebase 10. In a particular embodiment
as depicted in FIG. 13B, irregular granules of lysine freebase 10 may be
surrounded by a shell of lysine hydrochloride 20.

[0060]In another embodiment, the raspberry morphology as depicted in FIG.
13C includes several cores of irregular granules of lysine freebase 10
surrounded by a shell of threonine 40, or in an alternative embodiment
shown in FIG. 13D, cores of irregular granules threonine 40 surrounded by
a shell of lysine freebase 10.

[0061]A still further aspect of the present teaching is a composition
comprising lysine freebase, lysine hydrochloride or threonine granules
primarily of gradient morphology, that is, wherein the composition of the
particles gradually changes from the center to the surface of the
granule.

[0062]A further aspect of the present teaching is a composition comprising
lysine freebase, lysine hydrochloride or threonine granules primarily of
interpenetrating network morphology wherein there are two co-continuous
or co-centric shells of two different compositions creating an entangle.

[0063]A still further aspect of the present teaching is a composition
comprising lysine freebase, lysine hydrochloride or threonine granules
primarily of "salt-and-pepper" morphology wherein the particles are
composed of two or more different compositions that are in separate
domains.

[0064]Still another aspect of the present teaching is a composition
comprising lysine freebase, lysine hydrochloride or threonine granules
primarily of "ice-cream cone" morphology wherein two or more particles of
different compositions, share a surface of contact that may be large or
small.

[0066]A still further aspect of the present teaching is a composition
comprising lysine freebase, lysine hydrochloride or threonine granules
containing a combination of two or more morphologies mentioned above.
Some of the morphologies discussed above are illustrated in FIG. 14.

[0067]The various embodiments of the onion or raspberry morphology
described herein are understood to be non-limiting and one of ordinary
skill in the art may tailor them suitably to obtain a desired flow
behavior of the finished product.

[0069]According to other non-limiting embodiments, an aqueous solution of
lysine freebase may be used, which may comprise an aqueous solution
comprising from about 45% by weight to about 55% by weight of lysine
freebase. In other non-limiting embodiments, the lysine content of the
aqueous solution of lysine freebase may be increased as desired by either
removal or lowering the amount of water in the solution or by the
addition of an additional lysine product, such as a soluble salt of
lysine, for example, lysine HCl and/or lysine sulfate. Alternatively,
according to other non-limiting embodiments, the lysine content of the
aqueous solution of lysine freebase may be decreased as desired by the
addition of water to the solution.

[0070]A method for preparing the heteromorphic granules described in the
various embodiments of this disclosure is shown in the principle steps of
an inventive process in FIG. 15. The processes described herein may be
used to produce a lysine feed supplement with a final lysine purity in
the range theoretically between about 35% and 80%. Fermentation 200 may
be carried out by any suitable means described in the art such as for
instance as describe in U.S. Pat. No. 6,017,555 the contents of in which,
in their entirety are incorporated herein by reference.

[0071]After fermentation 200 a cell separation 21 may be used to separate
the biomass and obtain a substantially cell-free lysine broth 21B. The
cell free broth 21B is then processed through a chromatography step 22 to
obtain a purified lysine freebase stream 22A. The lysine freebase is may
then be subjected to evaporation 23 to increase its dry solids and
acidified using a mineral acid 25 in a crystallizer 30 to crystallize
salt of lysine, such as for example, lysine hydrochloride. The salt of
lysine may then be dried in dryer 32.

[0072]The salt of lysine 28 may have a purity in a range between about 35%
and 80% lysine, measured as a percent of freebase per kg. The lysine
broth from the cell separation step may also be, in one embodiment,
agglomerated with the salt of lysine by using a spray granulator 61 to
provide particles of lysine in the core with particles of lysine or
Threonine in the shell. The agglomerated particles, may also in one
embodiment, be sifted in sieve 62 to provide the final lysine feed
supplement 78. Oversized particles from sieve 62 may be processed through
a grinder 68 and be used as "recharge" material for spray granulator 61.

[0073]In an alternate embodiment of the inventive process shown in FIG.
15, the lysine freebase 40 used in the spray granulator 61 may be
obtained either from cell separation step 21, chromatography 22 or
evaporation 23.

[0074]In another alternative embodiment of the inventive process shown in
FIG. 16, the broth from fermentation 200 may be subjected to evaporation
50. After evaporation to increase its dry solids, the product may be
acidified 51 using a mineral acid 60. The acidified product may then be
dried 52 using techniques known in the art such as, but not limited to
drum drying, spray drying, vacuum tray drying, vacuum belt drying etc. to
obtain salts of lysine 53 which may serve as raw material for spray
granulator 61.

[0075]In another embodiment threonine 29 (either freebase or a salt there
of) may be added to the spray granulator 61 to obtain either a shell or a
core containing the aforementioned amino acid.

[0076]In yet another embodiment threonine 29 may be replaced with any
other suitable amino acid either in freebase form, or a salt there of,
such as tryptophan, methionine etc.

[0077]In another embodiment sieve 62 and grinder 68 may be used to obtain
an agglomerated product of the desired particle size.

[0078]In on aspect of this disclosure lysine freebase 400 may be obtained
from any one of streams 36, 37 or 38. In one embodiment of this
disclosure lysine freebase 400 may be mixed with small quantities of acid
such that the stream 400 may be a mixture of lysine freebase and a salt
of lysine.

[0079]In one aspect of this disclosure commercially available liquid
lysine may be used as a base core in spray co-agglomeration with a lysine
salt shell In one embodiment, the Liquid lysine® brand lysine is an
approximately 50% (by weight) aqueous solution of lysine freebase
obtained by concentrating lysine from a lysine fermentation broth.

[0080]In another aspect lysine monohydrochloride (HCl) may be used as a
base core with a lysine freebase shell. lysine hydrochloride is
commercially available in the form of lysine hydrochloride from
Archer-Daniels-Midland Company, Decatur, Ill. Lysine hydrochloride may be
obtained from, for example, but not limited to, purifying the product of
a lysine fermentation process by crystallization of the hydrochloride
salt. lysine hydrochloride (available from Archer-Daniels-Midland
Company, Decatur, Ill., as well as other suppliers) may be utilized
either as a granular solid or as an aqueous solution.

[0081]While another aspect of this disclosure is the harvesting and
processing of lysine base from fermentation broth, the composition and
nature of the fermentation medium may vary. For example, any suitable
high lysine producing organism taken from the genus E.Coli
Corynebacterium or Brevibacterium may be used to inoculate the
fermentation medium. The pH is adjusted and maintained at approximately
7.2 with ammonium hydroxide. The temperature is maintained at about 32
degree. C. The feed is Glucose and (NH4)2SO4 with the
glucose concentration initialized at about 10 g/l.

[0082]The fermentation medium can be inoculated into the fermentation
vessel by using standard microbiological practices which are known to
those skilled in the microbiology art. The fermentation vessel should be
equipped with a stirrer, a ventilation system, and a temperature control
device to maintain the fermentation at about 30 degree C. to about 32
degree C. The fermentation is carried out until the lysine base
concentration is about 92 g/l (grams per liter) and the total dry solids
is about 218 g/l. Aseptic techniques should be observed throughout the
fermentation process to avoid a contamination of the fermentation broth
with non-lysine producing organisms. The process produces a lysine feed
supplement in the form of a substantially dust free, free flowing,
granular lysine from fermentation broth comprising a salt of lysine
co-granulated with lysine freebase.

[0083]In another embodiment, the substantially cell free enriched lysine
broth is atomized by a nozzle 56 to provide an atomized spray of
substantially cell free enriched lysine broth to make a percolating bed
of lysine particulates in a spray granulator 61. The lysine particulates
have a particle size of less than about 177 micron (i.e. particles that
can pass through 80 mesh) and between the size range of about 100 micron
and 177 micron. The bed of the spray granulator may be a fluidized bed of
lysine particulates and is operated at a temperature between about 30
degrees C. and 100 degree C. The position of the nozzle 56 is adjusted
until it is just above the fluidized bed of lysine particulates.
Substantially cell free enriched lysine broth is sprayed onto the
fluidized bed of lysine particulates to initiate the agglomeration
process.

[0084]In an alternate embodiment a solution of lysine hydrochloride is
sprayed onto the fluidized bed of lysine particulates to initiate the
agglomeration process. In a yet another alternate embodiment a solution
of threonine is sprayed onto the fluidized bed of lysine particulates to
initiate the agglomeration process. In a further alternative embodiment a
solution of tryptophan is sprayed onto the fluidized bed of lysine
particulates to initiate the agglomeration process. The agglomeration
process is allowed to continue to produce the substantially dust free,
free flowing, granular lysine coated with a shell of lysine hydrochloride
or threonine or lysine freebase, in the size range between approximately
177 micron and 1190 micron, or in the size range of between about 177
micron to 420 micron. The product is then screened and sorted for size at
sieve 62 Granules at 62 that are too large (e.g. in the size range of
greater than about 1190 micron) are ground in a grinder at 68 to a
smaller particle size (e.g. in the size range of less than about 177
micron) and combined with material that is too small 84 (e.g. in the size
range of less than about 177 micron) to produce recycled lysine
particulates (shown "recharge" on FIGS. 14 and 15) and returned to the
spray granulator 61 as a starting material which act as seeds for the
agglomeration process. The substantially dust free, free flowing,
granular lysine product in the size range of about 177 micron to 1190
micron pass through the sieving process and are acceptable as the end
product at 78. However, a range is from about 177 micron to 420 micron
may be used which can pack better and reduces cost for shipment.

[0085]The lysine concentration in the lysine fermentation broth may be
about 90 g/l lysine to about 200 g/l lysine, measured as a percent of
freebase per kg. However, the lysine concentration can vary from one
fermentation run to the next. Hence, the use of a fermentation broth
containing about 90 g/l lysine means that other suitable concentrations
of lysine in the fermentation broth are acceptable. However, the lysine
concentration in the fermentation broth should not be below about 30 g/l.
Although ultrafiltration is the one method for obtaining the
substantially cell free lysine broth in step 21 in FIG. 13, this does not
mean other methods can not be used. The cells could also be removed by
mechanical separation techniques, such as centrifugation. Other suitable
methods include microfiltration and decanting.

[0086]This disclosure envisages the removal of cells from the lysine
containing fermentation broth by various other processes. For example,
the fermentation broth 20 could be split equally and about 50%
centrifuged and the remaining 50% ultrafiltered with the outputs from
both cell removal processes combined to produce a substantially cell free
lysine broth. This flexibility will enhance the practice of the invention
in an industrial setting. Although the present invention envisages the
addition of material containing lysine to the substantially cell free
concentrated lysine broth, the addition of such material to the
concentrated lysine broth might be omitted altogether if the desired
concentration of lysine (measured as freebase) is such that the addition
is unnecessary. For example, the step of adding a material containing
lysine might be omitted if the concentration of lysine in the
substantially cell free concentrated lysine broth substantially exceeds
about 35% lysine, measured as a percent of freebase per kg. If the cell
free concentrated lysine broth contains substantially more than about 35%
lysine, measured as a percent of freebase per kg, the lysine broth is a
substantially cell free enriched lysine broth.

[0087]Experience has shown that there is a relationship between the
orifice size of the nozzle 56, flow rate, and gauge pressure. While the
nozzle size may be 0.0615'', various other nozzles can also be used to
supply the spray. In particular, nozzle designs supplied by Spraying
Systems Co., PO Box 7900, Wheaton, Ill. 60189, USA work well to produce a
fine spray. The spray granulator can be purchased from Glatt Air
Techniques, 20 Spear Road, Ramsey, N.J. 07446-1288, USA.

[0088]Experience also suggests that manufacturing lysine granules on a
commercial scale will require several nozzles to atomize and spray
enriched lysine broth onto a proportionally larger bed of percolating
particles of lysine.

[0089]The percolating bed of particles should comprise lysine particles of
sufficiently small size to function as seeds for the agglomeration
process. The lysine particulates may be less than about 177 micron in
size and about 100 micron and 177 micron. In the agglomeration process,
the seed particles simultaneously grow in size and are dried as they are
sprayed with the enriched lysine permeate. The agglomeration process is
aided by various components which are inherently present in the enriched
lysine broth, namely: lysine fermentation broth, lysine hydrochloride,
lysine sulfate and water. Such components may act as binder and are
defined as substances which provide the sticky component to enable the
seeds in the agglomeration process to build up in size.

[0090]The source of the lysine particulates used to produce and seed the
fluidized bed of lysine in the spray granulator is not critical although
the source is either obtained from atomizing the substantially cell free
enriched lysine broth from step 53 in FIG. 15 or from recycled lysine
particulates (described as "recharge" in FIG. 15).

[0091]Alternatively, the fluidized bed of lysine particulates could be
produced by spray atomizing either a lysine containing fermentation
broth, a substantially cell free lysine broth, and substantially cell
free concentrated lysine broth or any mixture of these to produce a dry
powder of lysine granules. Another example of a suitable source of the
lysine particulates would be dry purified lysine hydrochloride powder and
lysine sulfate which has been dried to a powder. The source of lysine
particles may be sieved to remove lumps and sorted for particles less
than about 177 micron (The may be in the size range between about 100
micron and 177 micron).

[0092]Experience has shown that the agglomeration process becomes
self-sustaining by using the particles from recycling particles at 88 on
either a batch or semi-continuous basis.

[0093]lysine has a C to N ratio of 3:1 The lysine products according to
various non-limiting embodiments may comprise nitrogen content ranging
from about 9% N to about 20% N, depending of the formulation. In certain
embodiments, the nitrogen content of the lysine products may range from
about 9% N to about 15% N.

[0094]In another aspect of this disclosure, the products produced using
the embodiments described herein, may be used to produce fertilizer
compositions, such as, those described in co-pending applications U.S.
Provisional Application Ser. No. 60/726,749, filed Oct. 14, 2005, and
U.S. Provisional Application Ser. No. 60/789,051, filed Apr. 3, 2006, the
disclosures of which are incorporated in their entirety by reference
herein.

[0095]In yet another additional non-limiting embodiment, mineral or
mineral salts may be coated on the granules described herein to provide
N--P--K nutritional value to the granules for use as for instance but not
limited to animal feed, fertilizer, potting soil compositions, golf
greens and lawn fertilizers, horticultural and agricultural fertilizers
and mulches. Other suitable mineral or mineral salts include those
containing zinc, manganese, magnesium, calcium or iron that may be
combined alone or in combination with other minerals in the heteromorphic
lysine granule.

[0096]In an additional non-limiting embodiment, the compositions described
herein, may be produced at a first geographic location and transported or
shipped to a second geographic location. For instance, a facility at the
first geographic location may be able to produce a product more
economically than a facility at the second location due to various
factors. The factors may include, for example, lower costs of materials,
lower costs of energy (e.g., electricity and/or natural gas or other
petroleum products), lower costs of labor (e.g., wages paid to
employees), lower costs of environmental controls or effects, or any
other requirement for production of the compositions. Thus, the costs of
producing the products in the first geographic location may be less than
the costs of producing the products in the second geographic location,
resulting in the production costs being less in the first geographic
location.

[0097]In such an instance, the compositions may be produced at the first
geographic location and shipped to the second geographic location such as
by transport over water with ships or barges, trucking, flying, by rail,
or other means of transportation. The geographic location may be a
county, a state, a country, a continent, and/or combinations of any
thereof. In this manner the product may be produced, for example, in a
first county, state, country, or continent, and transported to and/or
sold in a second county, state, country, or continent.

[0098]The examples below are only representative of some aspects of this
disclosure. It will be understood by those skilled in the art that
processes as set forth in the specification can be practiced with a
variety of alterations with the benefit of the disclosure. These examples
and the procedures used therein should not be interpreted as limiting
this disclosure in any way not explicitly stated in the claims.

[0100]Three different process intermediate from the lysine manufacturing
process described in FIGS. 15-16 are utilized as raw materials.

[0101](a) Liquid lysine solutions with a nominal lysine concentration of
50% (Stream "A") but with an allowable range of 20% -80% solids.

[0102](b) lysine hydrochloride solution that is used to feed the lysine
hydrochloride crystallization step as described in FIG. 1 (Stream "B").

[0103](c) Dry lysine hydrochloride final product (Stream "C")

[0104]The various feed streams (A, B, or C) may be used to produce an
amino acid product as follows:

[0105](1) Starting with a sample from the Stream "A", the product is dried
to produce a liquid lysine powder with the desired moisture content.

[0106](2) Starting with a sample from the Stream "A", the product is
evaporated to raise the dry solids concentration and dried to obtain a
free flowing lysine powder.

[0107](3) Sample of Streams "A" and "B" is blended and dried to a desired
moisture level.

[0108](4) Sample of Streams "A" and "B" is blended and evaporated to a
higher solids concentration. The evaporated product is dried to obtain a
free flowing lysine powder

[0109](5) The product from tests 1 and 2 is spray coated with lysine
hydrochloride using a spray agglomerator type dryer.

[0110](6) The product from Stream "C" is spray coated with Stream "A"
using a spray agglomerator type dryer.

[0111](7) The products from tests 1-6, either by them selves or in
combination is dry blended with Stream "C".

[0112](8) The product of Stream "A" is pH adjusted to a target of 2.0-12.0
and dried to the desired moisture content.

[0113](9) The product of Stream "A" is pH adjusted to a target of 2.0-12.0
and evaporated to raise the dry solids and dried to obtain a free flowing
lysine powder.

EXAMPLE 2

[0114]RUN 2: In this Embodiment Coating on Lysine HCl of Lysine Freebase
was Studied.

[0115]A solution of 90 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 10 parts by
volume of lysine mother liquor (35 from FIG. 15) containing 50.8 percent
dry solids and 320.4 g/l lysine freebase on a lysine HCL recharge using a
spray granulator. An initial recharge of 250 g product was used. The
inlet dryer temperature was kept at 275° F. and bed temperature
was between 180° to 185° F. Feed was preheated to a
temperature of 160° F. ad the dryer was sprayed at rates to keep
the outlet temp greater than 159° F. Spray agglomeration was
initially started at 8 ml/min for first 15 minutes and gradually
increased to 20 ml/min as outlet temperatures permitted. A total of 1800
ml of lysine freebase and 900 ml of lysine HCL were used. Spray
agglomeration was continued until the weight of the bed reached 1.5 kg
where in product was recovered, sieved and analyzed. Results are
presented in Tables 1-3.

EXAMPLE 3

[0116]RUN 3: In this Embodiment Effect of Coating Lysine and Threonine
Freebase on Lysine Salts was Studied.

[0117]A solution of 60 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 40 parts by
volume of threonine ultrafiltration concentrate blend containing 70
percent dry solids and 120 g/l threonine freebase on a lysine HCL
recharge using a spray granulator. An initial recharge of 250 g product
was used. The inlet dryer temperature was kept at 70° C. and bed
temperature was between 150-170 degrees F. Feed was preheated to a
temperature of 100° F. ad the dryer was sprayed at rates to keep
the outlet temp greater than 159° F. Spray agglomeration was
initially started at 8 ml/min for first 15 minutes and gradually
increased to 15 ml/min as outlet temperatures permitted. Spray
agglomeration was continued until the weight of the bed reached 1.5 kg
wherein product was recovered, sieved and analyzed. Results are presented
in Tables 1-3.

EXAMPLE 4

[0118]RUN 4: In this Embodiment Effect of Coating Lysine Freebase on
Lysine Salts was Studied.

[0119]A solution of 80 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 20 parts by
volume of lysine freebase ultrafiltration concentrate blend containing 50
percent dry solids and 250 g/l lysine freebase on a lysine HCL recharge
using a spray granulator. An initial recharge of 800 g product was used.
The inlet dryer temperature was kept at 148 C and bed temperature was
between 150-170 degrees F. Feed was preheated to a temperature of 71 C ad
the dryer was sprayed at rates to keep the outlet temp greater than 148
C. Spray agglomeration was initially started at 8 ml/min for first 15
minutes and gradually increased to 15 ml/min as outlet temperatures
permitted. A total volume of 2000 ml feed was sprayed. Spray
agglomeration was continued until the weight of the bed reached 1.3 kg
where in product was recovered, sieved and analyzed. Results are
presented in Tables 1-3.

EXAMPLE 5

[0120]RUN 5: In this Embodiment Effect of Coating Lysine Freebase and
Lysine UF Concentrate on Lysine Salts was Studied.

[0121]A solution of 50 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 50 parts by
volume of lysine freebase ultrafiltration concentrate blend containing 50
percent dry solids and 250 g/l lysine freebase on a lysine HCL recharge
using a spray granulator. An initial recharge of 800 g product was used.
The inlet dryer temperature was kept at 148 C and bed temperature was
between 150-170 degrees F. Feed was preheated to a temperature of 71 C ad
the dryer was sprayed at rates to keep the outlet temp greater than 148
C. Spray agglomeration was initially started at 8 ml/min for first 15
minutes and gradually increased to 15 ml/min as outlet temperatures
permitted. A total volume of 2000 ml feed was sprayed. Spray
agglomeration was continued until the weight of the bed reached 1.3 kg
where in product was recovered, sieved and analyzed. Results are
presented in Tables 1-3.

EXAMPLE 6

[0122]RUN 6: In this Embodiment Effect of Coating Lysine Freebase and
Lysine Mother Liquor on Lysine Salts was Studied.

[0123]A solution of 91 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 9 parts by
volume of lysine freebase mother liquor containing 48.3 percent dry
solids and 320.4 g/l lysine freebase on a lysine HCL recharge using a
spray granulator. An initial recharge of 400 g product was used. The
inlet dryer temperature was kept at 148 C and bed temperature was between
150-170 degrees F. Feed was preheated to a temperature of 71 C ad the
dryer was sprayed at rates to keep the outlet temp greater than 148 C.
Spray agglomeration was initially started at 8 ml/min for first 15
minutes and gradually increased to 15 ml/min as outlet temperatures
permitted. A total volume of 1850 ml feed was sprayed. Spray
agglomeration was continued until the weight of the bed reached 1.915 kg
where in product was recovered, sieved and analyzed. Results are
presented in Tables 1-3.

EXAMPLE 7

[0124]RUN 7: In this Embodiment Effect of Coating Lysine Freebase and
Lysine Mother Liquor on Lysine Salts was Studied.

[0125]A solution of 90 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 10 parts by
volume of lysine freebase mother liquor containing 44 percent dry solids
and 320.4 g/l lysine freebase on a lysine HCL recharge using a spray
granulator. An initial recharge of 400 g product was used. The inlet
dryer temperature was kept at 70 C and bed temperature was between
140-160 degrees C. Feed was preheated to a temperature of 37.7 C ad the
dryer was sprayed at rates to keep the outlet temp greater than 70 C.
Spray agglomeration was initially started at 8 ml/min for first 15
minutes and gradually increased to 15 ml/min as outlet temperatures
permitted. A total volume of 1800 ml feed was sprayed. Spray
agglomeration was continued until the weight of the bed reached 1.915 kg
where in product was recovered, sieved and analyzed. Results are
presented in Tables 1-3.

EXAMPLE 8

[0126]RUN 6: In this Embodiment Effect of Coating Lysine Freebase and
Lysine Mother Liquor on Lysine Salts was Studied.

[0127]A solution of 91 parts by volume of 725 g/l lysine freebase
containing 70 percent dry solids was co-sprayed a solution of 1 part by
volume of lysine freebase mother liquor containing 48.3 percent dry
solids and 320.4 g/l lysine freebase on a lysine HCL recharge using a
spray granulator. An initial recharge of 400 g product was used. The
inlet dryer temperature was kept at 148 C and bed temperature was between
140-170 degrees C. Feed was preheated to a temperature of 71 C ad the
dryer was sprayed at rates to keep the outlet temp greater than 148 C.
Spray agglomeration was initially started at 8 ml/min for first 15
minutes and gradually increased to 15 ml/min as outlet temperatures
permitted. A total volume of 1850 ml feed was sprayed. Spray
agglomeration was continued until the weight of the bed reached 1.915 kg
where in product was recovered, sieved and analyzed. Results are
presented in Tables 1-3.

[0128]In this embodiment caking tests on lysine granules prepared
according to the various embodiments of this disclosure are performed.

[0129]A sample of 10.0 grams of product prepared according to various
embodiments of this disclosure is stored in a glass vial and is exposed
to various relative humidity conditions for 7 days before evacuation.
Upon evacuation the products are examined visually a relative scale:

[0130]0=Flowed Easily, no clumps.

[0131]1=Needed a gentle tap to initiate flow.

[0132]2=Needed a sharp tap to initiate flow.

[0133]3=Solid cake.

[0134]4=Laden with water.

[0135]The caking tests are performed under the following conditions.

[0136]A. Relative humidity 33%, Temperature 30 degrees C.

[0137]B. Relative humidity 51%, Temperature 30 degrees C.

[0138]C. Relative humidity 63%, Temperature 30 degrees C.

[0139]D. Relative humidity 72.8%, Temperature 30 degrees C.

[0140]E. Relative humidity 84%, Temperature 30 degrees C.

[0141]F. Relative humidity 91%, Temperature 30 degrees C.

[0142]The granules prepared according to the various aspects of this
disclosure are found to rate 0 or 1 on the relative scale indicating good
flowability.

[0143]Specific methods and compositions described herein are
representative of preferred embodiments and are exemplary and not
intended as limitations on the scope of the invention. Other objects,
aspects, and embodiments will occur to those skilled in the art upon
consideration of this specification, and are encompassed within the
spirit of the invention as defined by the scope of the claims. Where
examples are given, the description shall be construed to include but not
to be limited to only those examples. It will be readily apparent to one
skilled in the art that varying substitutions and modifications may be
made to the invention disclosed herein without departing from the scope
and spirit of the invention, and from the description of the inventions,
including those illustratively set forth herein, it is manifest that
various modifications and equivalents can be used to implement the
concepts of the present invention without departing from its scope. A
person of ordinary skill in the art will recognize that changes can be
made in form and detail without departing from the spirit and the scope
of the invention. The described embodiments are to be considered in all
respects as illustrative and not restrictive. Thus, for example,
additional embodiments are within the scope of the disclosure and within
the following claims.

Patent applications by Kenneth E. Tague, Mt. Zion, IL US

Patent applications by Kevin Moore, Mt. Zion, IL US

Patent applications by Sundeep N. Vani, Champaign, IL US

Patent applications in class CONTAINING NON-PROTEINACEOUS NITROGEN SOURCE CONVERTIBLE TO AVAILABLE NITROGEN OR PROCESS OF PREPARATION

Patent applications in all subclasses CONTAINING NON-PROTEINACEOUS NITROGEN SOURCE CONVERTIBLE TO AVAILABLE NITROGEN OR PROCESS OF PREPARATION